CN102449192B - Electroless palladium plating solution - Google Patents
Electroless palladium plating solution Download PDFInfo
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- CN102449192B CN102449192B CN2010800237515A CN201080023751A CN102449192B CN 102449192 B CN102449192 B CN 102449192B CN 2010800237515 A CN2010800237515 A CN 2010800237515A CN 201080023751 A CN201080023751 A CN 201080023751A CN 102449192 B CN102449192 B CN 102449192B
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- Prior art keywords
- palladium
- compound
- plating solution
- plating
- electrolysis
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Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/42—Coating with noble metals
- C23C18/44—Coating with noble metals using reducing agents
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/12—Mountings, e.g. non-detachable insulating substrates
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/48—Arrangements for conducting electric current to or from the solid state body in operation, e.g. leads, terminal arrangements ; Selection of materials therefor
- H01L23/50—Arrangements for conducting electric current to or from the solid state body in operation, e.g. leads, terminal arrangements ; Selection of materials therefor for integrated circuit devices, e.g. power bus, number of leads
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/10—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern
- H05K3/18—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using precipitation techniques to apply the conductive material
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/22—Secondary treatment of printed circuits
- H05K3/24—Reinforcing the conductive pattern
- H05K3/244—Finish plating of conductors, especially of copper conductors, e.g. for pads or lands
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
- H01L2224/80—Methods for connecting semiconductor or other solid state bodies using means for bonding being attached to, or being formed on, the surface to be connected
- H01L2224/85—Methods for connecting semiconductor or other solid state bodies using means for bonding being attached to, or being formed on, the surface to be connected using a wire connector
- H01L2224/8538—Bonding interfaces outside the semiconductor or solid-state body
- H01L2224/85399—Material
- H01L2224/854—Material with a principal constituent of the material being a metal or a metalloid, e.g. boron (B), silicon (Si), germanium (Ge), arsenic (As), antimony (Sb), tellurium (Te) and polonium (Po), and alloys thereof
- H01L2224/85463—Material with a principal constituent of the material being a metal or a metalloid, e.g. boron (B), silicon (Si), germanium (Ge), arsenic (As), antimony (Sb), tellurium (Te) and polonium (Po), and alloys thereof the principal constituent melting at a temperature of greater than 1550°C
- H01L2224/85464—Palladium (Pd) as principal constituent
Abstract
Disclosed is an electroless palladium plating solution which can form a plating layer having excellent soldering properties onto electronic components and the like and excellent wire bonding properties. The electroless palladium plating solution comprises a palladium compound, an amine compound, an inorganic sulfur compound and a reducing agent, wherein a combination of hypophosphorous acid or a hypophosphorous acid compound and formic acid or a formic acid compound is used as the reducing agent, and wherein the palladium compound, the amine compound, the inorganic sulfur compound, the hypophosphorous acid compound, and formic acid or the formic acid compound are contained in amounts of 0.001 to 0.1 mole/l, 0.05 to 5 moles/l, 0.01 to 0.1 mole/l, 0.05 to 1.0 mole/l and 0.001 to 0.1 mole/l, respectively. The electroless palladium plating solution is characterized by having excellent soldering properties and excellent wire bonding properties.
Description
Technical field
The present invention relates to as the soldering installation of electronic unit etc. and wire-bonded are used with plating without electrolysis Pd-P alloys plating bath.
Background technology
All the time, for substrate and the electronic unit with independent circuits is installed, use electroless nickel plating/electroless plating gold process.
In recent years, require to suppress the local corrosion of nickel plating tunicle owing to circuit complicated.In addition, because rising suddenly and sharply of price of gold lattice also makes an urgent demand of the cost that reduces electronic unit etc. increase.Thereupon, the technology of the thickness of the various electroless plating palladiums of enforcement, reduction electroless gold plating tunicle causes concern between electroless nickel plating and electroless gold plating.
For the such technology of correspondence, proposed without electrolysis Pd-P alloys plating bath and without the pure palladium plating solution of electrolysis.
But, with regard to existing without with regard to the electrolysis Pd-P alloys plating bath, because plating Induction time (to the time of plating reaction beginning) is long, it is slow to demonstrate speed of separating out, follow the complicated of plating circuit, produce the tendency of not plating palladium partly and then showing the meltage increase of electroless plating nickel flashing when plating palladium, the problem that produces the nickel local corrosion.
On the other hand, with regard to regard to the pure palladium plating solution of electrolysis because the plating palladium tunicle of separating out is crystalline material, therefore with electroless plating Pd-P alloys tunicle relatively, the easy thermodiffusion that becomes of gold-plated tunicle and plating palladium tunicle.Therefore, the bad difficult problem of wire-bonded characteristic after existing the high-melting-point soldering to install.
The prior art document
Patent documentation
Patent documentation 1: Japanese JP 03-1382 communique
Patent documentation 2: Japanese kokai publication sho 62-124280 communique
Patent documentation 3: Japanese kokai publication hei 05-39580 communique
Patent documentation 4: TOHKEMY 2001-3179 communique
Patent documentation 5: TOHKEMY 2007-92092 communique
Patent documentation 6: Japanese kokai publication hei 08-269727 communique
Patent documentation 7: No. 3035763 communique of Japanese Patent
Patent documentation 8: No. 4117016 communique of Japanese Patent
Summary of the invention
The problem that invention will solve
With regard to regard to the pure palladium plating solution of electrolysis because the plating palladium tunicle of separating out is crystalline material, therefore with electroless plating palladium-phosphorus tunicle relatively, the easy thermodiffusion that becomes of gold-plated tunicle and plating palladium tunicle.Therefore, the wire-bonded characteristic after the high-melting-point soldering is installed is poor.
The object of the present invention is to provide the electroless plating palladium Induction time (induction time) that shortens on nickel flashing even, separate out excellent in stability, the nickel meltage when suppressing the plating palladium in the situation of implementing the mounting conditions such as high-melting-point soldering installation, also have excellent scolding tin characteristic and wire-bonded characteristic without the electrolysis palladium plating solution.
Solve the means of problem
The inventor concentrates on studies in order to overcome described problem, found that, in the plating bath of the inorganic sulfide compound that comprises the complexing agent, selected from mercapto acetic acid, thiodiglycolic acid, Sulfothiorine and the S-WAT that are selected from palladium compound, amine and used the reductive agent that is selected from the Hypophosporous Acid, 50 compound and be selected from formic acid or the reductive agent of formate improves as the plating Induction time without electrolysis palladium-phosphor bath of reductive agent, the nickel stripping quantity during the plating palladium is inhibited.In addition, with regard to the palladium tunicle of separating out, be improved as the thermodiffusion between the gold-palladium after installing without the high-melting-point soldering of the difficult problem of the pure plating palladium of electrolysis tunicle.Can form the plating tunicle of various scolding tin characteristics and wire-bonded excellence by these fact-findings, thereby finish the present invention.
Namely, the present invention relates to without the electrolysis palladium plating solution, it is characterized in that, the inorganic sulfide compound 0.01～0.1mol/l that comprises palladium compound 0.001～0.1mol/l, amine compound 0.05～5mol/l, selected from mercapto acetic acid, thiodiglycolic acid, Sulfothiorine and S-WAT and reductive agent without the electrolysis palladium plating solution in, as described reductive agent and with the reductive agent 0.05～1.0mol/l that is selected from the Hypophosporous Acid, 50 compound be selected from the reductive agent 0.001～0.1mol/l of formic acid or formic acid cpds.
The invention effect
Of the present invention without the electrolysis palladium plating solution owing to bathe excellent in stability, therefore can be by the supply of palladium compound and reductive agent long-time the use.
As reductive agent and used the reductive agent that is selected from Hypophosporous Acid, 50 and be selected from the reductive agent of formic acid or formic acid cpds, so the Induction time that electroless plating covers shortens, and can prevent from plating the phenomenon of not separating out of palladium tunicle.
The plating palladium tunicle that obtains contains phosphorus, therefore becomes the palladium tunicle with fine crystalline.And, even in the situation of using high-melting-point scolding tin to install, also be difficult to occur the thermodiffusion of gold-plated-palladium tunicle, and after installing, the high-melting-point soldering obtains excellent wire-bonded characteristic.
Embodiment
Below, the present invention is described in detail.
As enumerating known palladium compound at the palladium compound that uses in without the electrolysis palladium plating solution of the present invention.Particularly, such as enumerating: Palladous chloride, palladium, Palladous nitrate, palladous sulfate, ammonium platinic chloride etc.
The palladium concentration of above-mentioned palladium compound is 0.001～0.1mol/l, is preferably 0.005～0.05mol/l.Palladium concentration is that speed of separating out reduces in the following situation of 0.001mol/l, causes that therefore not separating out of palladium, palladium concentration are 0.1mol/l when above, and solution stability is impaired, so not preferred.
As at the Hypophosporous Acid, 50 compound that uses in without the electrolysis palladium plating solution of the present invention, such as enumerating: sodium hypophosphite, potassium hypophosphite, ammonium hypophosphite etc.Above-mentioned Hypophosporous Acid, 50 compound works as main reductive agent and to the phosphorous segregation source of palladium tunicle in the palladium evolution reaction, and its concentration is 0.01～1mol/l, is preferably 0.05～0.7mol/l.The concentration of Hypophosporous Acid, 50 compound is that speed of separating out reduces in the following situation of 0.01mol/l, causes that palladium do not separate out, and the concentration of Hypophosporous Acid, 50 compound is that solution stability is impaired, so not preferred in the above situation of 1mol/l.
Then, as the amine compound at the complexing agent that uses in without the electrolysis palladium plating solution of the present invention, can enumerate: methylamine, dimethyl amine, Trimethylamine, benzylamine, methylene diamine, quadrol, tetramethylene-diamine, diethylenetriamine, EDTA, EDETATE SODIUM, tetren etc. can use a kind of these amine compound or and with more than 2 kinds.
Its usage quantity is 0.01～5mol/l, is preferably 0.03～3mol/l.
In the present invention, in order to improve bath stability and to separate out stability, add known inorganic sulfide compound.
Particularly, can enumerate: Thiovanic acid, thiodiglycolic acid, Sulfothiorine, S-WAT etc.
The addition of above-mentioned inorganic sulfide compound is 0.01～10mol/l, be preferably 0.03～5mol/l.Under it is situation below the 0.01mol/l, can not get above-mentioned effect, it is 10mol/l when above, speed of separating out reduces, and the undecomposed phenomenon of palladium occurs.
And then, of the present invention will be selected from the reductive agent of Hypophosporous Acid, 50 compound in without the electrolysis palladium plating solution and be selected from formic acid, sodium formiate, potassium formiate and ammonium formiate etc. reductive agent and with and compounding.
Above-mentioned formic acid or formate performance are assisted as the reduction reaction of the Hypophosporous Acid, 50 compound of main reductive agent and are prevented the undecomposed effect of palladium.
The usage quantity of above-mentioned formic acid or formic acid cpds is 0.001～0.1mol/l, is preferably 0.003～0.05mol/l.It is 0.001mol/l when following, and the ability of the reduction reaction of auxiliary Hypophosporous Acid, 50 compound is low, therefore the undecomposed phenomenon of palladium can occur, and under it was situation more than the 0.1mol/l, bath stability was impaired, so not preferred.
Of the present invention without the usually use under 35～80 ℃ of electrolysis palladium plating solution, but preferably 40～70 ℃ of lower uses.Plating temperature is in the situation below 35 ℃, and speed of separating out reduces, and is not preferred in the practicality.In addition, plating temperature is that solution stability is impaired, so not preferred in the situation more than 80 ℃.
In addition, of the present invention during without the electrolysis palladium plating solution in management, in the pH of plating bath is 4.0～10.0 scope, uses, preferably use in the scope 5.0～8.0.
The pH of plating bath is in the situation below 4.0, and the stability of the complex compound of palladium and amine compound reduces, so not preferred.In addition, under the pH of plating bath was situation more than 10, the stability of the complex compound of palladium and amine compound improved, but as the Hypophosporous Acid, 50 compound of main reductive agent and and usefulness as the formic acid of reductive agent or the reducing power grow of formic acid cpds, therefore solution stability is impaired, so not preferred.In addition, the pH of above-mentioned plating bath adjusts according to conventional methods in the alkali aqueous solutions such as the acidic aqueous solution such as sulfuric acid, phosphoric acid or sodium hydroxide and gets final product.
Below, enumerate embodiment and further the present invention is described in detail, but only otherwise exceed its main idea, the present invention just is not limited to following embodiment.
Embodiment 1
Embodiment 2
Embodiment 3
Comparative example 1
Comparative example 2
Comparative example 3
Comparative example 4
Comparative example 5
Evaluation method
Preparation above-described embodiment, comparative example without the electrolysis palladium plating solution, each sample is implemented electroless nickel plating/electroless plating palladium/electroless gold plating, compare test with following evaluation method.To the results are shown in table 1.
The liquid stability test
The 100ml beaker that drops into each palladium plating solution is impregnated into is warming up to 90 ℃ thermostatic bath, investigation liquid stability.
Separate out property testing
The electroless plating nickel flashing of the about 3 μ m of film forming carried out washing step after 90 seconds on the printed circuit board (PCB) that conduction electrode and independent micro-electrode mix, and implemented the electroless plating palladium, the one-tenth membrane stage of investigation plating palladium tunicle.
Tin soldering wettability
Implement electroless nickel plating (3 μ m), electroless plating palladium (0.1 μ m) and electroless gold plating (0.08 μ m) at 25 * 25mm copper coin, investigate tin soldering wettability with high-melting-point scolding tin.
Wire-bonded
Implement plating (the plating condition is same as described above) to estimating with sample, under the condition identical with high-melting-point scolding tin, after refluxing, utilize the joint of gold thread, investigation wire-bonded strength characteristics.
In this case, to estimate as benchmark without electrolytic nickel (5 μ m)/electroless gold plating (0.5 μ m).
[table 1]
According to the above results, hypophosphite being used as the first reductive agent without the electrolysis palladium plating solution of embodiments of the invention used formic acid or formate, therefore as the second reductive agent, plating palladium tunicle becomes fine and close, even and also can access good wire-bonded after high-melting-point scolding tin refluxes.
On the other hand, do not use the comparative example 1 of formic acid or formate and comparative example 2 wire-bonded good although use hypophosphite, bath poor stability and speed of separating out are slow, therefore produce the undecomposed phenomenon of palladium in absolute electrode section.
In addition, do not use the comparative example 3 of hypophosphite to bathe although use sodium formiate and have good stability, do not produce Pd and separate out badly, wire-bonded is bad.
The bath poor stability of comparative example 4 and comparative example 5, its tin soldering wettability and wire-bonded all fail to measure.
Industrial utilizability
Without for the electrolysis palladium plating solution, its tin soldering wettability, wire-bonded are excellent for of the present invention, so its applicability to the substrate that has the high-melting-point soldering and install is high.
Claims (5)
1. without the electrolysis palladium plating solution, comprise palladium compound, amine compound, sulphur compound and reductive agent, it is characterized in that following (a) and (b),
(a) contain the described sulphur compound that 0.01～0.1mol/l measures, its selected from mercapto acetic acid, thiodiglycolic acid, Sulfothiorine and S-WAT,
(b) described reductive agent and be that the Hypophosporous Acid, 50 of amount of 0.05～1.0mol/l or hypophosphite and content are formic acid or the formate of the amount of 0.001～0.1mol/l with content.
2. according to claim 1ly it is characterized in that without the electrolysis palladium plating solution that palladium compound is to be selected from Palladous chloride, palladium, Palladous nitrate, palladous sulfate and the ammonium platinic chloride one or more.
3. according to claim 1 without the electrolysis palladium plating solution, it is characterized in that amine compound is to be selected from methylamine, dimethyl amine, Trimethylamine, benzylamine, methylene diamine, quadrol, tetramethylene-diamine, diethylenetriamine, EDTA, EDETATE SODIUM and the tetren one or more.
4. according to claim 1ly it is characterized in that without the electrolysis palladium plating solution pH value without the electrolysis palladium plating solution of claim 1 is 4.0～10.0.
5. according to claim 1ly it is characterized in that without the electrolysis palladium plating solution temperature without the electrolysis palladium plating solution of claim 1 is 35～80 ℃.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2009-113655 | 2009-05-08 | ||
| JP2009113655A JP4511623B1 (en) | 2009-05-08 | 2009-05-08 | Electroless palladium plating solution |
| PCT/JP2010/058150 WO2010128688A1 (en) | 2009-05-08 | 2010-05-07 | Electroless palladium plating solution |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102449192A CN102449192A (en) | 2012-05-09 |
| CN102449192B true CN102449192B (en) | 2013-10-30 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2010800237515A Active CN102449192B (en) | 2009-05-08 | 2010-05-07 | Electroless palladium plating solution |
Country Status (6)
| Country | Link |
|---|---|
| US (1) | US8562727B2 (en) |
| JP (1) | JP4511623B1 (en) |
| KR (1) | KR101351230B1 (en) |
| CN (1) | CN102449192B (en) |
| SG (1) | SG175937A1 (en) |
| WO (1) | WO2010128688A1 (en) |
Families Citing this family (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2581470B1 (en) * | 2011-10-12 | 2016-09-28 | ATOTECH Deutschland GmbH | Electroless palladium plating bath composition |
| JP2013253283A (en) * | 2012-06-06 | 2013-12-19 | Kanto Gakuin | Electroless plating bath |
| US20140072706A1 (en) * | 2012-09-11 | 2014-03-13 | Ernest Long | Direct Electroless Palladium Plating on Copper |
| CN103290399B (en) * | 2013-06-19 | 2015-09-30 | 广东东硕科技有限公司 | A kind of chemical palladium plating solution using one package stabilizer |
| KR101617654B1 (en) * | 2013-08-23 | 2016-05-03 | 숭실대학교 산학협력단 | Manufacturing method of palladium thin films using electroless-plating |
| CN103556140A (en) * | 2013-11-13 | 2014-02-05 | 北京达博有色金属焊料有限责任公司 | Palladium plating liquid for chemically preparing palladium-plated copper bonding wire |
| US9758874B2 (en) * | 2014-04-10 | 2017-09-12 | Atotech Deutschland Gmbh | Plating bath composition and method for electroless plating of palladium |
| KR102482321B1 (en) | 2014-09-04 | 2022-12-27 | 니혼 고쥰도가가쿠 가부시키가이샤 | Palladium plating solution and palladium coating obtained using same |
| CN104498918A (en) * | 2014-11-28 | 2015-04-08 | 广东致卓精密金属科技有限公司 | Chemical palladium plating solution for intermediate layer of chemical nickel, palladium and gold plating process |
| US20170321327A1 (en) * | 2014-12-17 | 2017-11-09 | Atotech Deutschland Gmbh | Plating bath composition and method for electroless plating of palladium |
| US9603258B2 (en) | 2015-08-05 | 2017-03-21 | Uyemura International Corporation | Composition and method for electroless plating of palladium phosphorus on copper, and a coated component therefrom |
| TWI692547B (en) | 2015-11-27 | 2020-05-01 | 德國艾托特克公司 | Plating bath composition and method for electroless plating of palladium |
| TW201922969A (en) | 2017-08-03 | 2019-06-16 | 美商電子墨水股份有限公司 | Conductive ink compositions comprising palladium and methods for making the same |
| JP7185999B2 (en) | 2017-10-06 | 2022-12-08 | 上村工業株式会社 | Electroless palladium plating solution |
| JP7149061B2 (en) * | 2017-10-06 | 2022-10-06 | 上村工業株式会社 | Electroless palladium plating solution |
| JP7407644B2 (en) | 2020-04-03 | 2024-01-04 | 上村工業株式会社 | Palladium plating solution and plating method |
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| CN101356299A (en) * | 2005-09-27 | 2009-01-28 | 上村工业株式会社 | Electroless palladium plating bath and electroless palladium plating method |
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| US3418143A (en) * | 1967-08-15 | 1968-12-24 | Burroughs Corp | Bath for the electroless deposition of palladium |
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- 2009-05-08 JP JP2009113655A patent/JP4511623B1/en active Active
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- 2010-05-07 KR KR1020117026533A patent/KR101351230B1/en active IP Right Grant
- 2010-05-07 US US13/319,194 patent/US8562727B2/en active Active
- 2010-05-07 WO PCT/JP2010/058150 patent/WO2010128688A1/en active Application Filing
- 2010-05-07 SG SG2011082039A patent/SG175937A1/en unknown
- 2010-05-07 CN CN2010800237515A patent/CN102449192B/en active Active
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| JP3972158B2 (en) * | 1998-03-24 | 2007-09-05 | 石原薬品株式会社 | Electroless palladium plating solution |
| CN101228293A (en) * | 2005-07-20 | 2008-07-23 | 日矿金属株式会社 | Plating solution for electroless palladium plating |
| CN101356299A (en) * | 2005-09-27 | 2009-01-28 | 上村工业株式会社 | Electroless palladium plating bath and electroless palladium plating method |
| JP2008291348A (en) * | 2007-04-27 | 2008-12-04 | Hitachi Chem Co Ltd | Connecting terminal, semiconductor package using connecting terminal, and method for manufacturing semiconductor package |
Also Published As
| Publication number | Publication date |
|---|---|
| US8562727B2 (en) | 2013-10-22 |
| SG175937A1 (en) | 2011-12-29 |
| KR101351230B1 (en) | 2014-01-13 |
| US20120118196A1 (en) | 2012-05-17 |
| JP2010261082A (en) | 2010-11-18 |
| WO2010128688A1 (en) | 2010-11-11 |
| CN102449192A (en) | 2012-05-09 |
| KR20120005498A (en) | 2012-01-16 |
| JP4511623B1 (en) | 2010-07-28 |
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